CN102964216A - Decyne glycol synthesizing technology - Google Patents
Decyne glycol synthesizing technology Download PDFInfo
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- CN102964216A CN102964216A CN2012105175821A CN201210517582A CN102964216A CN 102964216 A CN102964216 A CN 102964216A CN 2012105175821 A CN2012105175821 A CN 2012105175821A CN 201210517582 A CN201210517582 A CN 201210517582A CN 102964216 A CN102964216 A CN 102964216A
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Abstract
The invention relates to a decyne glycol synthesizing technology. The decyne glycol synthesizing technology is characterized by mainly comprising the following two steps of: A. neutralization: adding a catalyst and a solvent to a reaction kettle, uniformly stirring at the temperature of 20-50 DEG C, feeding acetylene, pumping methyl isobuty ketone 4-methyl-2-pentanon by a metering pump slowly first and faster afterwards after stable absorption, simultaneously carrying out reppe reaction, and skimming and neutralizing in a skimming tank after reaction for 6-8 hours; and B. rectification: adding a molten decyne glycol crude product to a rectifying column, reducing pressure and rectifying, and intercepting a main distillate fraction at the tower top temperature of 165-170 DEG C, wherein the reflux ratio is (5:1)-(10:1), and when the tower top temperature drops, the main fraction interception is ceased. In the step A, the acetylene is added at a nitrogen environment. The methyl isobuty ketone 4-methyl-2-pentanon is pumped by the metering pump slowly first and faster afterwards. The time of pumping the methyl isobuty ketone 4-methyl-2-pentanon by the metering pump lasts for 2-3 hours.
Description
Technical field
The present invention relates to a kind of tensio-active agent, especially a kind of synthesis technique of nonionic polyfunctional surfactant decynediol.
Background technology
The decynediol tensio-active agent is the water based systems nonionogenic tenside, can significantly reduce the surface tension of water.The decynediol polyfunctional surfactant usually is re-dubbed liquid with all kinds of SOLVENTS, with convenient use.Be used for water-borne coatings, dyestuff and the fields such as water color ink, agricultural chemicals, use very extensive.Can be used as wetting agent, the defoamer of water-borne coatings, improve homogeneity and the flowability of coating.But the by product of original processing condition one alkynol causes turnover ratio low, yield about 60%.
Summary of the invention
The defective that exists for solving prior art, the present invention's proposition can improve the technique of a kind of synthetic decynediol of transformation efficiency.
Realize purpose of the present invention, the technical solution used in the present invention is: a kind of technique of synthetic decynediol is characterized in that mainly containing following two steps:
A neutralizes: catalyzer and solvent are added in the reactor, stir under the temperature 20-50 ℃ of state, pass into and squeeze into hexone with volume pump after the acetylene absorption is stablized, the continuation reaction entering separatory tank separatory and neutralizing after 6-8 hour;
B, rectifying: add the decynediol crude product that melts in rectifying tower, rectification under vacuum is in tower top temperature 165-170 ℃ of lower intercepting main distillate fraction, reflux ratio 5; 1-10:1 stops to intercept main distillate fraction when tower top temperature begins to descend.The described adding acetylene of steps A is to add under nitrogen environment.Steps A is described squeezes into hexone with volume pump, begins simultaneously to carry out the reppe reaction, and beginning is slow, the later stage is fast.
The invention has the beneficial effects as follows: because in the situation of the control of the temperature of the technique of this synthetic decynediol and speed, it is few to reach side reaction, the transformation efficiency of product is high.
Description of drawings
Fig. 1 is process flow diagram of the present invention.
The present invention will be further described below in conjunction with embodiment and accompanying drawing.
Embodiment
Add 500 kilograms of methyl tertiary butyl ethers in 2 cubes of reactors, open about mixing speed 80r/min, room temperature adds 200 kilograms of potassium hydroxide powder.Close opening for feed, 10-20 ℃ of reactor cooling, the temperature of reactor is to be controlled by PLC.Use the nitrogen replacement air, replacing nitrogen 5 times repeatedly with acetylene.Opening the acetylene inlet valve keeps acetylene gas often to open.Be replaced the afterreaction still and be warming up to 20-50 ℃.Mixing speed transfers to about 120r/min, begins to squeeze into methyl iso-butyl ketone (MIBK) with volume pump, begins simultaneously to carry out reppe reaction, and is slow during beginning, the later stage is fast, approximately adds 200 kilograms of methyl iso-butyl ketone (MIBK) in 2-3 hour.Adding speed is controlled by volume pump P101.Continued logical acetylene 2-3 hour after adding methyl iso-butyl ketone (MIBK), until acetylene no longer absorbs.Reacted 6-8 hour, and then used nitrogen replacement.Be cooled to 10-20 ℃ and add 400 kilograms of distilled water stirrings 30 minutes.Open still bottom valve mixture and enter a minute flow container, static 60 minutes.Lower aqueous layer is discarded to the recycling of potassium hydroxide tank.The upper strata oil reservoir mixes with 200 kilograms of distilled water to stir with rotating speed 80r/min and neutralizes with glacial acetic acid after 30 minutes.Static 6-8 hour.Lower aqueous layer continues to put into the potassium hydroxide withdrawing can.
The upper strata oil reservoir is squeezed into rectifying tower.Under nitrogen protection, normal pressure slowly is warmed up to 90-100 ℃ and goes out to heat up in a steamer, and cut enters solvent recovery tank, until till not going out to heat up in a steamer.
Opening vacuum pump is evacuated down to 40mmHg begins to intercept main distillate fraction when about 165 ℃ of cat head.Reflux ratio 5:1 to 10:1, at the bottom of the still temperature 167-190 ℃, about 132 ℃ of rectifying tower epimere temperature, about 134 ℃ of hypomere temperature.Regulating 112 cuts enters and returns your pure finished pot of fault.When beginning to descend, tower top temperature stops to intercept main distillate fraction.Stopped heating blasts nitrogen, closes vacuum, changes emptying into, is cooled to below 100 ℃, and rectifying finishes.Product purity 〉=99%, yield about 70%.
Claims (4)
1. the technique of a synthetic decynediol is characterized in that mainly containing following steps:
A neutralizes: catalyzer and solvent are added in the reactor, stir under the temperature 20-50 ℃ of state, pass into and squeeze into hexone with volume pump after the acetylene absorption is stablized, the continuation reaction entering separatory tank separatory and neutralizing after 6-8 hour;
B, rectifying: add the decynediol crude product that melts in rectifying tower, rectification under vacuum is in tower top temperature 165-170 ℃ of lower intercepting main distillate fraction, reflux ratio 5; 1-10:1 stops to intercept main distillate fraction when tower top temperature begins to descend.
2. the technique of a kind of synthetic decynediol according to claim 1, it is characterized in that: the described adding acetylene of steps A is to add under nitrogen environment.
3. the technique of a kind of synthetic decynediol according to claim 1, it is characterized in that: steps A is described squeezes into hexone with volume pump, begins simultaneously to carry out the reppe reaction, and beginning is slow, the later stage is fast.
4. the technique of a kind of synthetic decynediol according to claim 1 is characterized in that: steps A is described, and to add the hexone time with volume pump be 2-3 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105175821A CN102964216A (en) | 2012-12-06 | 2012-12-06 | Decyne glycol synthesizing technology |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105175821A CN102964216A (en) | 2012-12-06 | 2012-12-06 | Decyne glycol synthesizing technology |
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| CN102964216A true CN102964216A (en) | 2013-03-13 |
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| CN2012105175821A Pending CN102964216A (en) | 2012-12-06 | 2012-12-06 | Decyne glycol synthesizing technology |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242140A (en) * | 2013-04-20 | 2013-08-14 | 岳阳市英泰合成材料有限公司 | Production method of acetylenic diol series products |
| CN103304376A (en) * | 2013-06-20 | 2013-09-18 | 重庆闽东化工有限责任公司 | Clean production process of alkyne diol serial products |
| CN106832247A (en) * | 2016-12-28 | 2017-06-13 | 杭州电化集团助剂化工有限公司 | A kind of production technology of polyfunctional surfactant tetramethyl decynediol ethoxy compound |
| CN108121317A (en) * | 2018-02-07 | 2018-06-05 | 重庆消烦多新材料有限公司 | A kind of ECS hot spot multiple unit control systems for preparing alkynol based compound |
| CN113816835A (en) * | 2021-09-27 | 2021-12-21 | 四川众邦制药有限公司 | Method for coproducing dimethyl decyne diol and methyl hexine alcohol |
| CN113880690A (en) * | 2021-09-27 | 2022-01-04 | 四川众邦制药有限公司 | Method for co-producing tetramethyl decyne diol and dimethyl hexine alcohol |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4960959A (en) * | 1987-04-04 | 1990-10-02 | Huels Aktiengesellschaft | Process for the manufacture of alkynediols by reaction of ketones with acetylene |
| US20030018221A1 (en) * | 2001-07-03 | 2003-01-23 | Hideki Omori | Process for continuous production of acetylenediol |
| CN102476978A (en) * | 2010-11-24 | 2012-05-30 | 杨朝辉 | Novel synthetic method preparing alkynol compound from acetylene |
-
2012
- 2012-12-06 CN CN2012105175821A patent/CN102964216A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4960959A (en) * | 1987-04-04 | 1990-10-02 | Huels Aktiengesellschaft | Process for the manufacture of alkynediols by reaction of ketones with acetylene |
| US20030018221A1 (en) * | 2001-07-03 | 2003-01-23 | Hideki Omori | Process for continuous production of acetylenediol |
| CN102476978A (en) * | 2010-11-24 | 2012-05-30 | 杨朝辉 | Novel synthetic method preparing alkynol compound from acetylene |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242140A (en) * | 2013-04-20 | 2013-08-14 | 岳阳市英泰合成材料有限公司 | Production method of acetylenic diol series products |
| CN103242140B (en) * | 2013-04-20 | 2015-07-29 | 岳阳市英泰合成材料有限公司 | A kind of production method of alkyne diol series product |
| CN103304376A (en) * | 2013-06-20 | 2013-09-18 | 重庆闽东化工有限责任公司 | Clean production process of alkyne diol serial products |
| CN106832247A (en) * | 2016-12-28 | 2017-06-13 | 杭州电化集团助剂化工有限公司 | A kind of production technology of polyfunctional surfactant tetramethyl decynediol ethoxy compound |
| CN108121317A (en) * | 2018-02-07 | 2018-06-05 | 重庆消烦多新材料有限公司 | A kind of ECS hot spot multiple unit control systems for preparing alkynol based compound |
| CN113816835A (en) * | 2021-09-27 | 2021-12-21 | 四川众邦制药有限公司 | Method for coproducing dimethyl decyne diol and methyl hexine alcohol |
| CN113880690A (en) * | 2021-09-27 | 2022-01-04 | 四川众邦制药有限公司 | Method for co-producing tetramethyl decyne diol and dimethyl hexine alcohol |
| CN113880690B (en) * | 2021-09-27 | 2024-03-15 | 四川众邦新材料股份有限公司 | Method for co-producing tetramethyl decynyl glycol and dimethyl hexynyl alcohol |
| CN113816835B (en) * | 2021-09-27 | 2024-04-12 | 四川众邦新材料股份有限公司 | Method for co-production of dimethyl decynediol and methyl hexynol |
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Application publication date: 20130313 |